ORGANOMETALLIC COMPOUNDS OF THE LANTHANIDES .59. (1,1'-(3-OXAPENTAMETHYLENE)DICYCLOPENTADIENYL)YTTRIUM AND -LUTETIUM 3,5-DIMETHYLPYRAZOLATES - X-RAY CRYSTAL-STRUCTURE OF [O(CH2CH2C5H4)2LN(MU-N2C3HME2)(MU-OH)LN(C5H4CH2CH2)2O] (LN = Y, LU)

被引：77

作者：

SCHUMANN, H ^{[1
]}

LOEBEL, J ^{[1
]}

PICKARDT, J ^{[1
]}

QIAN, CT ^{[1
]}

XIE, ZW ^{[1
]}

机构：

[1] CHINESE ACAD SCI,SHANGHAI INST ORGAN CHEM,SHANGHAI,PEOPLES R CHINA

来源：

ORGANOMETALLICS | 1991年 / 10卷 / 01期

关键词：

D O I：

10.1021/om00047a052

中图分类号：

O61 [无机化学];

学科分类号：

070301 ; 081704 ;

摘要：

The reaction of O(CH2CH2C5H4)2LnCl (Ln = Y, Lu) with NaN2C3HMe2 in tetrahydrofuran at room temperature generates the complexes O(CH2CH2C5H4)2Ln(N2C3HMe2) (Ln = Y (1), Lu (2)). The partial hydrolyses of 1 and 2 form [O(CH2CH2C5H4)2Ln(mu-N2C3HMe2)(mu-OH)Ln(C5H4CH2CH2)O] (Ln = Y (3), Lu (4)). The new compounds have been characterized by elemental analyses and IR and NMR spectra. The X-ray structural analyses of 3 and 4 show both to be tetragonal, space group P4(1)2(1)2, Z = 4, with a = 8.980 (2) angstrom, c = 37.403 (7) angstrom, and D(calcd) = 1.520 g cm-3 for 3 and a = 8.930 (5) angstrom, c = 36.868 (9) angstrom, and D(calcd) = 1.95 g cm-3 for 4. The structure was solved from 2294 observed reflections with F-degrees greater-than-or-equal-to 6-sigma-(F(o)) and refined to a final R factor of 0.0434 for 3 and from 2004 observed reflections with F(o) greater-than-or-equal-to a final R factor of 0.0323 for 4. The molecular structure shows the pyrazole and the hydroxyl groups both bridging with distances Y-N = 2.445 (5) angstrom, Y-O = 2.202 (2) angstrom, Lu-N = 2.392 (8) angstrom, and Lu-O = 2.154 (3) angstrom, whereas the oxygen atoms of the oxapentamethylene bridges are separated by 2.662 (4) angstrom from the Y atoms and 2.667 (7) angstrom from the Lu atoms.

引用

页码：215 / 219

页数：5

共 42 条

[21] ALKYL-BRIDGED COMPLEXES OF THE D-BLOCK AND F-BLOCK ELEMENTS .2. BIS-[BIS(ETA-CYCLOPENTADIENYL)METHYLMETAL(III)] COMPLEXES, AND THE CRYSTAL AND MOLECULAR-STRUCTURE OF THE YTTRIUM AND YTTERBIUM SPECIES [J].

HOLTON, J ;

LAPPERT, MF ;

BALLARD, DGH ;

PEARCE, R ;

ATWOOD, JL ;

HUNTER, WE .

JOURNAL OF THE CHEMICAL SOCIETY-DALTON TRANSACTIONS, 1979, (01) :54-61

[22] HIGHLY REACTIVE ORGANOLANTHANIDES - SYNTHESIS, CHEMISTRY, AND STRUCTURES OF 4F HYDROCARBYLS AND HYDRIDES WITH CHELATING BIS(POLYMETHYLCYCLOPENTADIENYL) LIGANDS [J].

JESKE, G ;

SCHOCK, LE ;

SWEPSTON, PN ;

SCHUMANN, H ;

MARKS, TJ .

JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1985, 107 (26) :8103-8110

[23] HIGHLY REACTIVE ORGANOLANTHANIDES - SYSTEMATIC ROUTES TO AND OLEFIN CHEMISTRY OF EARLY AND LATE BIS(PENTAMETHYLCYCLOPENTADIENYL) 4F HYDROCARBYL AND HYDRIDE COMPLEXES [J].

JESKE, G ;

LAUKE, H ;

MAUERMANN, H ;

SWEPSTON, PN ;

SCHUMANN, H ;

MARKS, TJ .

JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1985, 107 (26) :8091-8103

[24] SYNTHESIS OF NEW ORGANO DERIVATIVES OF EARLY LANTHANIDES [J].

JOHN, JN ;

TSUTSUI, M .

INORGANIC CHEMISTRY, 1981, 20 (05) :1602-1604

[25]

JOHNSON CK, 1965, ORNL3794 REP

[26] THE FORMATION AND X-RAY CRYSTAL-STRUCTURE OF (ETA-5-C5H5)2LUCL.OC4H8 [J].

NI, CZ ;

ZHANG, ZM ;

DENG, DL ;

QIAN, CT .

JOURNAL OF ORGANOMETALLIC CHEMISTRY, 1986, 306 (02) :209-214

[27] STUDIES ON ORGANOLANTHANIDE COMPLEXES .8. SYNTHESIS AND THERMAL-DECOMPOSITION OF NEW SIGMA-BONDED 1,1'-TRIMETHYLENEDICYCLOPENTADIENYL-EARLY LANTHANIDE COMPLEXES [J].

QIAN, CT ;

YE, CQ ;

LI, YQ .

JOURNAL OF ORGANOMETALLIC CHEMISTRY, 1986, 302 (02) :171-179

[28]

QIAN CT, 1987, INORG CHIM ACTA, V139, P195

[29] STUDIES ON ORGANOLANTHANIDE COMPLEXES .3. THE STABILIZATION OF EARLY LANTHANOCENE CHLORIDES BY USING A RING-BRIDGED DICYCLOPENTADIENE LIGAND [J].

QIAN, CT ;

YE, CQ ;

LU, HZ ;

LI, YQ ;

HUANG, YZ .

JOURNAL OF ORGANOMETALLIC CHEMISTRY, 1984, 263 (03) :333-343

[30] STUDIES ON ORGANOLANTHANIDE COMPLEXES .12. SYNTHESIS, IDENTIFICATION AND REACTIVITY OF ORGANOLANTHANIDE AND ORGANOYTTRIUM CHLORIDES WITH THE CHELATING 1,1'-(3-OXA-PENTAMETHYLENE)DICYCLOPENTADIENYL LIGAND [J].

QIAN, CT ;

XIE, ZW ;

HUANG, YZ .

JOURNAL OF ORGANOMETALLIC CHEMISTRY, 1987, 323 (03) :285-294

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